Lithium → (4,4-Difluorocyclohexyl)methanamine

4,4-difluorocyclohexanecarboxamide (1.32 g, 8.10 mmol) was stirred in the solution of lithium borohydrate (1M, 30 ml) under nitrogen overnight. Then, the reaction mixture was refluxed for 4 hours. After cooled to room temperature, it was poured into ice-water slowly. After filtration, the product was extracted with dichloromethane from filtrate. Combined organic layers were water, brine, dried over anhydrous sodium sulphate, filtered and condensed to provide a 934 mg of colorless oil (82%). δ 2.53 (d, 2H), 1.98-2.09 (m, 2H), 1.73-1.82 (m, 6H), 1.17-1.29 (m, 3H).

1. temperatureThen, the reaction mixture was refluxed for 4 hours
2. filtrationAfter filtration
3. extractionthe product was extracted with dichloromethane from filtrate
4. dry with materialdried over anhydrous sodium sulphate
5. filtrationfiltered
6. customcondensed

ORDレコード

ord-792faac33c954fd99d272d282b37b9a1

出典データセット

uspto-grants-2011_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07868008B2